WO2011026933A1 - Method for continuously separating organic materials of interest from fermentation - Google Patents

Method for continuously separating organic materials of interest from fermentation Download PDF

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Publication number
WO2011026933A1
WO2011026933A1 PCT/EP2010/062933 EP2010062933W WO2011026933A1 WO 2011026933 A1 WO2011026933 A1 WO 2011026933A1 EP 2010062933 W EP2010062933 W EP 2010062933W WO 2011026933 A1 WO2011026933 A1 WO 2011026933A1
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WIPO (PCT)
Prior art keywords
fermenter
fermentation
separation
biomass
flash evaporation
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PCT/EP2010/062933
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French (fr)
Inventor
Joël Schwartz
Philippe Marion
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Rhodia Operations
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Publication date
Application filed by Rhodia Operations filed Critical Rhodia Operations
Priority to US13/394,329 priority Critical patent/US20120220003A1/en
Priority to BR112012004770A priority patent/BR112012004770A2/en
Priority to CN2010800393123A priority patent/CN102482691A/en
Priority to EP10750118A priority patent/EP2473612A1/en
Publication of WO2011026933A1 publication Critical patent/WO2011026933A1/en

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    • C—CHEMISTRY; METALLURGY
    • C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
    • C12P7/00—Preparation of oxygen-containing organic compounds
    • C12P7/02—Preparation of oxygen-containing organic compounds containing a hydroxy group
    • C12P7/04—Preparation of oxygen-containing organic compounds containing a hydroxy group acyclic
    • C12P7/16—Butanols
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/001—Processes specially adapted for distillation or rectification of fermented solutions
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/001—Processes specially adapted for distillation or rectification of fermented solutions
    • B01D3/002—Processes specially adapted for distillation or rectification of fermented solutions by continuous methods
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/06—Flash distillation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D5/00—Condensation of vapours; Recovering volatile solvents by condensation
    • B01D5/0057—Condensation of vapours; Recovering volatile solvents by condensation in combination with other processes
    • B01D5/006—Condensation of vapours; Recovering volatile solvents by condensation in combination with other processes with evaporation or distillation
    • C—CHEMISTRY; METALLURGY
    • C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
    • C12P7/00—Preparation of oxygen-containing organic compounds
    • C12P7/02—Preparation of oxygen-containing organic compounds containing a hydroxy group
    • C12P7/04—Preparation of oxygen-containing organic compounds containing a hydroxy group acyclic
    • C12P7/06—Ethanol, i.e. non-beverage
    • C—CHEMISTRY; METALLURGY
    • C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
    • C12P7/00—Preparation of oxygen-containing organic compounds
    • C12P7/40—Preparation of oxygen-containing organic compounds containing a carboxyl group including Peroxycarboxylic acids
    • C12P7/56—Lactic acid
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E50/00—Technologies for the production of fuel of non-fossil origin
    • Y02E50/10—Biofuels, e.g. bio-diesel

Definitions

  • the present invention relates to a process for the continuous separation of organic products of interest from a fermentation, in particular lactic or alcoholic fermentation, by flash evaporation. This process makes it possible in particular not to inhibit the fermentation reaction and obtain very good yields and productivities.
  • liquid / liquid extractions or separations can be carried out using an absorbent such as activated carbon.
  • an absorbent such as activated carbon.
  • the thermodynamics is very favorable and that the adsorbent does not deliver toxic substances. It is also necessary to consider the desorption and washing phases, this solution is often complex for use on an industrial scale.
  • the Applicant has developed a process for separating the organic products of interest resulting from the fermentation consisting in continuously withdrawing fermentation must from the fermenter and then going to separate (stripper) the organic compounds of interest in an apparatus dissociated from the fermenter , and in particular recycling the feet of the separator to the fermenter. This is especially done by a relaxation of the must in a flash pot working under vacuum.
  • the organic compounds are flashed and entrained with water, in feet of the flash pot the must cooled by the evaporation of the solvents and water is recycled to the fermenter at a temperature such that it absorbs the exotherm of the fermentation.
  • the pressure is adjusted so as to obtain the temperature giving the thermal equilibrium to the fermenter. According to the needs, we bring calories to the flash.
  • the present invention thus has for its main object a method of continuously separating the organic products from a fermentation in a fermenter comprising at least the following steps:
  • step b) flash evaporation of the liquid separated in step b), and obtaining in the gaseous phase of the organic products
  • the process is preferably carried out continuously or semi-continuously.
  • fermentation is meant a biochemical reaction of conversion of the chemical energy contained in a carbon source, in particular glucose, into another form of energy directly usable by the cell, in particular in the absence of oxygen.
  • the fermentation according to the invention relates in particular to lactic fermentation and preferably to alcoholic fermentation which is the result of a metabolic chain which converts fermentable sugars, in particular yeasts, into alcohol and carbon dioxide with the release of heat.
  • the fermentation according to the invention leads to the production of the organic products of interest.
  • biomass means all living materials, usually microorganisms, present in the fermentation medium.
  • the fermenter used according to the present invention is a technological unit in which microorganisms, such as yeasts, bacteria, microscopic fungi, algae, or animal or plant cells, are multiplied for the bioconversion of an organic molecule of interest.
  • This bioreactor generally controls the culture conditions such as temperature, pH, and aeration. In the fermenter, the temperature is generally between 30 and 45 ° C.
  • the separation of the biomass is generally carried out in step b) before flash evaporation of step c).
  • filtration, ultrafiltration, decantation, centrifugation and / or ultracentrifugation can be carried out.
  • the arrival of the mill in the system allowing the flash evaporation is preferably carried out in an area having a pressure equivalent to or equal to the pressure of the fermenter.
  • the barometric height can allow a pressure gradient between 0.5 and 1 bar.
  • the circulation of the mout can for example be carried out by a pump.
  • the liquid obtained, also called liquid separated in step b), corresponds to the wort as defined previously essentially free of biomass.
  • This liquid generally has the same temperature as that of the fermenter.
  • the filtrate liquid is conveyed to the flash evaporation stage and the residue or retentate is returned to the fermenter.
  • Tangential ultrafiltration systems are generally used on an external pressure circulation loop. These ultrafiltration systems, with a cut-off threshold of the order of 0.01 ⁇ generally, usually operate under PTM transmembrane pressures of the order of 1 to 3 bar.
  • the sizing of such an ultrafiltration system depends on the quantity of organic products to be extracted from the reactor and the duration during which this extraction must be made. These parameters determine the volume of filtrate to be produced for flash evaporation.
  • the circulation rate of the wort inside the ultrafiltration module is generally between 2 and 5 m / s.
  • the membranes used are generally tubular mineral type having the advantage of being able to undergo effective cleaning treatments and be insensitive to clogging.
  • the flash evaporation of step c), or flash flash consists of placing the liquid in a vacuum tank, in particular with a pressure of between 0.001 and 0.9 bar. Vacuuming lowers the saturation temperature and evaporates some of the liquid. The evaporation will be done by taking energy from the mixture and thus cool it.
  • the vacuum flash evaporation process has been widely used for several decades in various industries. It is found in various applications such as desalination of seawater, the concentration and pasteurization of milk or the treatment of wastewater loaded with soluble oils.
  • a gas-liquid separator such as a flash tank or expansion tank, also called a flash pot.
  • a heat exchanger can be added in or next to the gas-liquid separator, depending on the needs energy, to heat or cool the flash evaporation medium.
  • a tubular or plate exchanger may be used.
  • the gas-liquid separator is generally a cylinder with a vertical axis. It comprises, for example, a liquid inlet pipe for the fermenter, an outlet at the base and an outlet at the head.
  • the column height may be a function of the desired barometric height as previously explained.
  • the gas-liquid separator may comprise a lining or trays so as to have a few theoretical stages of separation.
  • the flash evaporation is preferably carried out at a pressure of between 10 and 200 mbar.
  • the temperature during flash evaporation is generally between 10 and 40 ° C.
  • the vaporization rate may be between 1 and 70% by weight, preferably between 30 and 60% by weight.
  • This separation is preferably carried out without adding any particular external solvent to the compounds resulting from the fermentation.
  • the gaseous phase resulting from flash evaporation thus comprises the organic products of interest as well as incondensable dissolved substances such as CO2, H 2 . and CH 4 .
  • the gaseous phase is preferably brought to a condensing means, such as a condenser, in particular to separate the residual incondensables organic products of interest.
  • a condensing means such as a condenser
  • the aqueous phase resulting from the flash evaporation generally comprises water in large quantities and a minority of organic compounds.
  • This phase The aqueous solution is preferably recycled to the fermenter, and is especially at a temperature below the temperature of the fermenter, generally a temperature of 5 to 20 ° C lower than the temperature of the fermenter.
  • the organic products of interest of the gaseous phase are then isolated by one or more separation techniques known from the state of the art, such as in particular by distillation, liquid-liquid extraction, crystallization and / or adsorption. When the boiling temperatures are very close, it may be advantageous to use a fractional distillation process which consists of several successive refinement steps. It is also possible to introduce part of the distillate at the top of the column in the case of a continuous distillation in order to improve the purity of the vapor phase.
  • Some vapors of the gaseous phase may in particular be recondensed and the condensates may possibly be reintroduced into the fermenter.
  • Some or all of the gas phase water from flash separation can be condensed and recycled to the fermenter.
  • the water required for driving all the organic products produced in the fermenter is generally recycled.
  • the process according to the present invention is particularly suitable for the separation of biobutanol resulting from the fermentation of sugar cane molasses.
  • the gaseous phase of step c) generally comprises CO 2 , H 2 , azeotrope / butanol / water, water, acetone and ethanol; the liquid phase of the flash essentially consisting of water.
  • the process according to the present invention is also suitable for the separation of the ethanol resulting from the fermentation.
  • the present invention also covers devices for implementing the method according to the invention.
  • a preferred device corresponds to that of Figure 1 and comprises in particular a fermenter (2) provided with an arrival of nutrients, gas, musts and the like (1) and a means of evacuation of the mout (3).
  • the mout is routed to a biomass separation means (4), such as an ultrafiltration module.
  • the biomass is returned to the fermenter (2) by a suitable conveying means (8).
  • the fermentation liquor freed of its biomass is sent to the flash evaporation system (5), such as a gas-liquid separator (5).
  • the liquid phase is conveyed to the fermenter (2) by a suitable means (7) and the gas phase is then discharged to a condenser (6) which separates the remaining non-condensable organic products of interest. These will then be isolated by one or more conventional separation techniques.
  • a part of the liquid can be refluxed towards the head of the gas-liquid separator (5).
  • the device tested corresponds to that of Figure 1 and comprises in particular a fermenter (2) with a capacity of 1000 m 3 and operating at a temperature of 38 ° C.
  • the fermenter includes green juice concentrated with sugar cane at the beginning of fermentation.
  • the separation means (4) used is a tangential ultrafiltration module.
  • the system of flash evaporation is a gas-liquid separator (5) of flash pot type.
  • the liquid phase is fed to the fermenter (2) by a suitable means (7) and the gas phase is then discharged to a condenser (6). Part of the condensed water of the gas phase, discarded organic products is sent to the fermenter for recycling.
  • the production cycle is 200 hours.
  • the flow rate at the outlet of the ultrafiltration is adjusted so that for example 90% of the mass is recycled to the fermenter by means (8) and 10% of the mass passes through the membranes of the ultrafiltration module (4). .
  • the flash separation is carried out at a temperature of 30 ° C and a pressure in the gas phase of 0.045 bar.

Abstract

The present invention relates to a method for continuously separating organic materials of interest from fermentation, in particular lactic or alcoholic fermentation, by flash evaporation. Said method in particular makes it possible to avoid inhibiting the fermentation reaction and to obtain very high yields and productivity.

Description

Procédé de séparation en continu  Continuous separation process
des produits organiques d'intérêt d'une fermentation  organic products of interest of a fermentation
La présente invention concerne un procédé de séparation en continu des produits organiques d'intérêt d'une fermentation, notamment lactique ou alcoolique, par évaporation flash. Ce procédé permet notamment de ne pas inhiber la réaction de fermentation et obtenir de très bons rendements et productivités. ART ANTERIEUR The present invention relates to a process for the continuous separation of organic products of interest from a fermentation, in particular lactic or alcoholic fermentation, by flash evaporation. This process makes it possible in particular not to inhibit the fermentation reaction and obtain very good yields and productivities. PRIOR ART
Les procédés industriels de fermentation, notamment lactique et alcoolique, sont bien connus et permettent la fabrication de produits organiques d'intérêts qui peuvent être utilisés pour diverses applications. II se pose souvent le problème de l'isolation des produits organiques d'intérêts issus de la fermentation et notamment leur séparation de la biomasse.  Industrial fermentation processes, particularly lactic and alcoholic, are well known and allow the manufacture of organic products of interest that can be used for various applications. There is often the problem of isolating organic products of interest resulting from fermentation and in particular their separation from biomass.
On peut notamment procéder à des extractions liquide/liquide ou des séparations en utilisant un absorbant comme le charbon actif. Toutefois pour l'extraction liquide/liquide, il faut trouver un solvant qui présente un très bon coefficient de partage entre la phase aqueuse et la phase organique, et si l'on souhaite recycler la phase aqueuse au fermenteur pour améliorer rendement et productivité, que ce solvant ne soit pas un inhibiteur de la fermentation et si possible qui soit très peu soluble dans la phase aqueuse. Cela reste rarement le cas. Pour le traitement avec un adsorbant, il faut là aussi que la thermodynamique soit très favorable et que l'adsorbant ne délivre pas de substances toxiques. Il faut par ailleurs considérer les phases de désorption et de lavage, cette solution est souvent complexe pour une utilisation à l'échelle industrielle. II serait également possible de procéder à un stripping des produits organiques d'intérêts, notamment avec les incondensables générés lors de le fermentation, tels que le dioxyde de carbone, le méthane et l'hydrogène. Toutefois, cela s'avère très complexe dans la mesure où la température de fermentation avoisine les 30 ou 40°C et qu'à cette température il est rigoureusement impossible de stripper entièrement et de façon simple les composés organiques et l'eau avec les incondensables générés à la fermentation. Il serait donc nécessaire de recycler ces incondensables par un gros compresseur de gaz, des systèmes d'agitation dans des fermenteurs complexes pour disperser ces gaz, des systèmes de condensation démesurés avec des groupes frigorifiques de manière à piéger efficacement les composés organiques. Et ceci sans augmenter la température ni diminuer la pression dans le fermenteur pour ne pas endommager les microorganismes et diminuer le rendement des réactions d'intérêts. In particular, liquid / liquid extractions or separations can be carried out using an absorbent such as activated carbon. However for the liquid / liquid extraction, it is necessary to find a solvent which has a very good partition coefficient between the aqueous phase and the organic phase, and if it is desired to recycle the aqueous phase to the fermenter to improve yield and productivity, that this solvent is not an inhibitor of fermentation and if possible which is very slightly soluble in the aqueous phase. This is rarely the case. For the treatment with an adsorbent, it is also necessary that the thermodynamics is very favorable and that the adsorbent does not deliver toxic substances. It is also necessary to consider the desorption and washing phases, this solution is often complex for use on an industrial scale. It would also be possible to stripping organic products of interest, especially with the non-condensables generated during fermentation, such as carbon dioxide, methane and hydrogen. However, this is very complex since the fermentation temperature is around 30 or 40 ° C and that at this temperature it is strictly impossible to stripper completely and in a simple way the organic compounds and water with the incondensables generated during fermentation. It would therefore be necessary to recycle these incondensables by a large gas compressor, stirring systems in complex fermenters to disperse these gases, excessive condensation systems with refrigeration units so as to effectively trap organic compounds. And this without increasing the temperature or reducing the pressure in the fermenter to not damage the microorganisms and reduce the yield of interest reactions.
Il existait ainsi un besoin de mettre au point un procédé fiable et réaliste industriellement permettant de séparer efficacement les produits organiques d'intérêts issus de la fermentation tout en évitant les inconvénients mentionnés précédemment. There was thus a need to develop a reliable and industrially realistic process for effectively separating organic products of interest from fermentation while avoiding the disadvantages mentioned above.
INVENTION INVENTION
La demanderesse a mis au point un procédé de séparation des produits organiques d'intérêts issus de la fermentation consistant à soutirer en continu du moût de fermentation du fermenteur pour ensuite aller séparer (stripper) les composés organiques d'intérêts dans un appareil dissocié du fermenteur, puis notamment recycler les pieds du séparateur au fermenteur. Ceci est notamment effectué par une détente du moût dans un pot de flash travaillant sous vide. Les composés organiques sont flashés et entraînés avec de l'eau, en pieds du pot de flash le moût refroidi par l'évaporation des solvants et de l'eau est recyclé au fermenteur à une température telle qu'elle absorbe l'exothermie de la fermentation. Au pot de flash la pression est réglée de manière à obtenir la température donnant l'équilibre thermique au fermenteur. Suivant les besoins on apporte des calories au flash. Pour éviter l'inconvénient de la fragilité des microorganismes qui risquent d'éclater au moment du flash la biomasse est séparée avant le flash, par exemple par ultrafiltration ; le retentât étant directement renvoyé au fermenteur, le filtrat au flash. Cette solution technique permet ainsi d'éviter l'introduction des incondensables dans le fermenteur et donc de se passer de l'utilisation de compresseur ou de dispositif d'agitation complexe dans le fermenteur. Ceci permet également d'éviter l'utilisation d'échangeur thermique dans le fermenteur, puisque que l'on assure l'équilibre thermique avec le recyclage du pied de flash refroidi ; et donc de simplifier la technologie du fermenteur qui ne requiert plus d'échangeur interne et de système d'agitation. Ce procédé permet notamment de ne pas inhiber la réaction de fermentation et obtenir de très bons rendements et productivités. The Applicant has developed a process for separating the organic products of interest resulting from the fermentation consisting in continuously withdrawing fermentation must from the fermenter and then going to separate (stripper) the organic compounds of interest in an apparatus dissociated from the fermenter , and in particular recycling the feet of the separator to the fermenter. This is especially done by a relaxation of the must in a flash pot working under vacuum. The organic compounds are flashed and entrained with water, in feet of the flash pot the must cooled by the evaporation of the solvents and water is recycled to the fermenter at a temperature such that it absorbs the exotherm of the fermentation. At the flash pot the pressure is adjusted so as to obtain the temperature giving the thermal equilibrium to the fermenter. According to the needs, we bring calories to the flash. To avoid the disadvantage of the fragility of microorganisms that may burst at the time of flash biomass is separated before the flash, for example by ultrafiltration; the retentate being returned directly to the fermenter, the filtrate flash. This technical solution thus makes it possible to prevent the introduction of incondensables into the fermenter and thus to dispense with the use of compressor or complex stirring device in the fermenter. This also makes it possible to avoid the use of a heat exchanger in the fermenter, since the thermal balance is ensured with the recycling of the cooled flash foot; and therefore to simplify the fermenter technology that no longer requires internal exchanger and stirring system. This process makes it possible in particular not to inhibit the fermentation reaction and obtain very good yields and productivities.
La présente invention a ainsi pour principal objet un procédé de séparation en continu des produits organiques d'une fermentation dans un fermenteur comprenant au moins les étapes suivantes : The present invention thus has for its main object a method of continuously separating the organic products from a fermentation in a fermenter comprising at least the following steps:
a) prélèvement en cours de fermentation, d'une partie du moût du fermenteur ; b) séparation de la biomasse qui est renvoyée au fermenteur ; a) sampling during fermentation of part of the fermentor must; (b) separation of the biomass returned to the fermenter;
c) évaporation flash du liquide séparé à l'étape b), et obtention en phase gazeuse des produits organiques ; et c) flash evaporation of the liquid separated in step b), and obtaining in the gaseous phase of the organic products; and
d) isolation des produits organiques. Le procédé est préférentiellement réalisé en continu ou semi-continu. d) insulation of organic products. The process is preferably carried out continuously or semi-continuously.
On entend par « fermentation », une réaction biochimique de conversion de l'énergie chimique contenue dans une source de carbone, notamment le glucose, en une autre forme d'énergie directement utilisable par la cellule, notamment en l'absence de dioxygène. La fermentation selon l'invention concerne notamment la fermentation lactique et préférentiellement la fermentation alcoolique qui est le résultat d'une chaîne métabolique qui transforme des sucres fermentescibles, notamment par des levures, en alcool et gaz carbonique avec dégagement de chaleur. La fermentation selon l'invention conduit à la production des produits organiques dits d'intérêts. On entend par « moût » de fermentation, le milieu de la réaction comprenant notamment la biomasse, les produits fermentescibles et les produits organiques obtenus par la fermentation. On entend par « biomasse » l'ensemble des matières vivantes, généralement les microorganismes, présents dans le milieu de fermentation. By "fermentation" is meant a biochemical reaction of conversion of the chemical energy contained in a carbon source, in particular glucose, into another form of energy directly usable by the cell, in particular in the absence of oxygen. The fermentation according to the invention relates in particular to lactic fermentation and preferably to alcoholic fermentation which is the result of a metabolic chain which converts fermentable sugars, in particular yeasts, into alcohol and carbon dioxide with the release of heat. The fermentation according to the invention leads to the production of the organic products of interest. The term "must" for fermentation, the reaction medium including biomass, fermentable products and organic products obtained by fermentation. The term "biomass" means all living materials, usually microorganisms, present in the fermentation medium.
Le fermenteur utilisé selon la présente invention est une unité technologique dans laquelle on multiplie des micro-organismes, comme les levures, bactéries, champignons microscopiques, algues, ou cellules animales ou végétales, pour la bioconversion d'une molécule organique d'intérêt. Ce bioréacteur permet généralement de contrôler les conditions de culture telles que la température, le pH, et l'aération. Dans le fermenteur, la température est généralement comprise entre 30 et 45°C. The fermenter used according to the present invention is a technological unit in which microorganisms, such as yeasts, bacteria, microscopic fungi, algae, or animal or plant cells, are multiplied for the bioconversion of an organic molecule of interest. This bioreactor generally controls the culture conditions such as temperature, pH, and aeration. In the fermenter, the temperature is generally between 30 and 45 ° C.
La séparation de la biomasse est généralement effectuée à l'étape b) avant d'effectuer l'évaporation flash de l'étape c). On peut par exemple procéder à une filtration, une ultrafiltration, une décantation, une centrifugation et/ou une ultracentrifugation. On peut également procéder à la séparation de la biomasse dans le séparateur gaz liquide utilisé pour effectuer l'évaporation flash, notamment en disposant une hauteur barométrique de liquide dans le séparateur gaz liquide de manière a éviter le choc de dépressurisation des micro-organismes lors de l'évaporation flash. Dans ce cas, l'arrivée du mout dans le système permettant l'évaporation flash est préférentiellement effectuée dans une zone ayant une pression équivalente ou égale à la pression du fermenteur. La hauteur barométrique peut permettre un gradient de pression compris entre 0,5 et 1 bar. The separation of the biomass is generally carried out in step b) before flash evaporation of step c). For example, filtration, ultrafiltration, decantation, centrifugation and / or ultracentrifugation can be carried out. It is also possible to separate the biomass in the liquid gas separator used to carry out the flash evaporation, in particular by placing a barometric height of liquid in the liquid gas separator so as to avoid the shock of depressurization of the microorganisms during flash evaporation. In this case, the arrival of the mill in the system allowing the flash evaporation is preferably carried out in an area having a pressure equivalent to or equal to the pressure of the fermenter. The barometric height can allow a pressure gradient between 0.5 and 1 bar.
La circulation du mout peut par exemple être effectuée par une pompe. Le liquide obtenu, également appelé liquide séparé à l'étape b), correspond au moût tel que défini précédemment essentiellement débarrassé de la biomasse. Ce liquide présente généralement la même température que celle du fermenteur. Dans le cas de l'ultrafiltration particulièrement préféré selon l'invention, le liquide filtrat est acheminé vers l'étape d'évaporation flash et le résidu ou retentât est renvoyée au fermenteur. On utilise généralement des systèmes d'ultrafiltration tangentielle sur une boucle de circulation externe sous pression. Ces systèmes d'ultrafiltration, d'un seuil de coupure de l'ordre de 0,01 μιτι généralement, fonctionnent habituellement sous des pression transmembranaires PTM de l'ordre de 1 à 3 bar. Le dimensionnement d'un tel système d'ultrafiltration dépend de la quantité de produits organiques a extraire du réacteur et de la durée pendant laquelle cette extraction doit être faite. Ces paramètres déterminent le volume de filtrat à produire en vue d'un évaporation flash. Le volume de filtrat à produire et la durée pendant laquelle le filtrat doit être produit, i.e. le temps de fonctionnement du système d'ultrafiltration, détermine la surface de membrane à installer. Les débits de filtration sont usuellement compris entre 20 et 100 l/m2.h. selon les caractéristiques du moût de fermentation et la PTM appliquée. La vitesse de circulation du moût à l'intérieur du module d'ultrafiltration est comprise généralement entre 2 et 5 m/s. Les membranes utilisées sont généralement de type minérale tubulaire présentant l'avantage de pouvoir subir des traitements de nettoyage efficace et être peu sensible au colmatage. L'évaporation flash de l'étape c), ou flash détente, consiste à placer le liquide dans une cuve sous vide, notamment avec une pression comprise entre 0,001 et 0,9 bar. La mise sous vide permet d'abaisser la température de saturation et d'évaporer une partie du liquide. L'évaporation va se faire en prenant de l'énergie au mélange et ainsi le refroidir. Le procédé d'évaporation flash sous vide est très largement utilisé depuis plusieurs décennies dans diverses industries. On le retrouve dans différentes applications telles que le dessalement de l'eau de mer, la concentration et la pasteurisation du lait ou le traitement des eaux usées chargées en huiles solubles. On peut a cet effet utiliser par exemple un séparateur gaz-liquide, comme une cuve de détente ou pot de détente, également appelé pot de flash. On peut également utiliser une ou plusieurs cuves de détente notamment à des pressions différentes. Un échangeur de chaleur peut être adjoint dans ou a coté du séparateur gaz-liquide, suivant les nécessités en apport énergétique, pour réchauffer ou refroidir le milieu de l'évaporation flash. On peut par exemple utiliser un échangeur tubulaire ou à plaques. The circulation of the mout can for example be carried out by a pump. The liquid obtained, also called liquid separated in step b), corresponds to the wort as defined previously essentially free of biomass. This liquid generally has the same temperature as that of the fermenter. In the case of the ultrafiltration particularly preferred according to the invention, the filtrate liquid is conveyed to the flash evaporation stage and the residue or retentate is returned to the fermenter. Tangential ultrafiltration systems are generally used on an external pressure circulation loop. These ultrafiltration systems, with a cut-off threshold of the order of 0.01 μιτι generally, usually operate under PTM transmembrane pressures of the order of 1 to 3 bar. The sizing of such an ultrafiltration system depends on the quantity of organic products to be extracted from the reactor and the duration during which this extraction must be made. These parameters determine the volume of filtrate to be produced for flash evaporation. The volume of filtrate to be produced and the time during which the filtrate is to be produced, ie the operating time of the ultrafiltration system, determines the membrane surface to be installed. Filtration rates are usually between 20 and 100 l / m 2 .h. depending on the characteristics of the fermentation must and the applied PTM. The circulation rate of the wort inside the ultrafiltration module is generally between 2 and 5 m / s. The membranes used are generally tubular mineral type having the advantage of being able to undergo effective cleaning treatments and be insensitive to clogging. The flash evaporation of step c), or flash flash, consists of placing the liquid in a vacuum tank, in particular with a pressure of between 0.001 and 0.9 bar. Vacuuming lowers the saturation temperature and evaporates some of the liquid. The evaporation will be done by taking energy from the mixture and thus cool it. The vacuum flash evaporation process has been widely used for several decades in various industries. It is found in various applications such as desalination of seawater, the concentration and pasteurization of milk or the treatment of wastewater loaded with soluble oils. For this purpose it is possible to use, for example, a gas-liquid separator, such as a flash tank or expansion tank, also called a flash pot. It is also possible to use one or more expansion tanks, in particular at different pressures. A heat exchanger can be added in or next to the gas-liquid separator, depending on the needs energy, to heat or cool the flash evaporation medium. For example, a tubular or plate exchanger may be used.
Le séparateur gaz-liquide est généralement un cylindre à axe vertical. Il comprend par exemple une tubulure d'arrivée du liquide du fermenteur, une sortie à la base et une sortie en tête. La hauteur de colonne peut être fonction de la hauteur barométrique souhaitée comme expliqué précédemment. The gas-liquid separator is generally a cylinder with a vertical axis. It comprises, for example, a liquid inlet pipe for the fermenter, an outlet at the base and an outlet at the head. The column height may be a function of the desired barometric height as previously explained.
Le séparateur gaz-liquide peut comporter un garnissage ou des plateaux de manière à avoir quelques étages théoriques de séparation. The gas-liquid separator may comprise a lining or trays so as to have a few theoretical stages of separation.
Selon la présente invention, l'évaporation flash est préférentiellement effectuée à une pression comprise entre 10 et 200 mbar. La température lors de l'évaporation flash est généralement comprise entre 10 et 40°C. According to the present invention, the flash evaporation is preferably carried out at a pressure of between 10 and 200 mbar. The temperature during flash evaporation is generally between 10 and 40 ° C.
Le taux de vaporisation peut être compris entre 1 et 70 % massique, préférentiellement entre 30 et 60 % massique. The vaporization rate may be between 1 and 70% by weight, preferably between 30 and 60% by weight.
Cette séparation est préférentiellement effectuée sans ajout de solvant particulier extérieur aux composés issus de la fermentation. This separation is preferably carried out without adding any particular external solvent to the compounds resulting from the fermentation.
La phase gazeuse issue de l'évaporation flash comprend ainsi les produits organiques d'intérêt ainsi que des incondensables dissous tels que le CO2, H2. et CH4. The gaseous phase resulting from flash evaporation thus comprises the organic products of interest as well as incondensable dissolved substances such as CO2, H 2 . and CH 4 .
La phase gazeuse est préférentiellement amenée à un moyen de condensation, tel qu'un condenseur, pour notamment séparer les incondensables résiduels des produits organiques d'intérêt. The gaseous phase is preferably brought to a condensing means, such as a condenser, in particular to separate the residual incondensables organic products of interest.
La phase aqueuse issue de l'évaporation flash comprend généralement de l'eau en fortes quantités et une minorité de composés organiques. Cette phase aqueuse est préférentiellement recyclée au fermenteur, et est notamment à une température inférieure à la température du fermenteur, généralement une température inférieure de 5 à 20°C par rapport à la température du fermenteur. Les produits organiques d'intérêt de la phase gazeuse sont alors isolés par une ou plusieurs techniques de séparations connues de l'état de la technique, telles que notamment par distillation, extraction liquide-liquide, cristallisation et/ou adsorption. Lorsque les températures d'ébullition sont très voisines, on peut avoir intérêt à utiliser un processus de distillation fractionnée qui consiste en plusieurs étapes de raffinements successifs. Il est également possible d'introduire une partie du distillât en tête de colonne dans le cas d'une distillation continue afin d'améliorer la pureté de la phase vapeur. The aqueous phase resulting from the flash evaporation generally comprises water in large quantities and a minority of organic compounds. This phase The aqueous solution is preferably recycled to the fermenter, and is especially at a temperature below the temperature of the fermenter, generally a temperature of 5 to 20 ° C lower than the temperature of the fermenter. The organic products of interest of the gaseous phase are then isolated by one or more separation techniques known from the state of the art, such as in particular by distillation, liquid-liquid extraction, crystallization and / or adsorption. When the boiling temperatures are very close, it may be advantageous to use a fractional distillation process which consists of several successive refinement steps. It is also possible to introduce part of the distillate at the top of the column in the case of a continuous distillation in order to improve the purity of the vapor phase.
Certaines vapeurs de la phase gazeuses peuvent notamment être recondensées et les condensais peuvent éventuellement être réintroduits dans le fermenteur. Une partie ou la totalité de l'eau de la phase gazeuse issue de la séparation flash peut être condensée et recyclée au fermenteur. On recycle généralement l'eau nécessaire à l'entraînement de la totalité des produits organiques produits dans le fermenteur. On peut notamment utiliser à cet effet des condenseurs à tubes, à plaques ou spiralés. Some vapors of the gaseous phase may in particular be recondensed and the condensates may possibly be reintroduced into the fermenter. Some or all of the gas phase water from flash separation can be condensed and recycled to the fermenter. The water required for driving all the organic products produced in the fermenter is generally recycled. In particular, it is possible to use tube, plate or spiral condensers for this purpose.
Le procédé selon la présente invention convient particulièrement pour la séparation du biobutanol issue de la fermentation des mélasses de cannes a sucre. Dans ce cas, la phase gazeuse de l'étape c) comprend généralement du CO2, de l'H2, de l'hétéro azéotrope butanol/eau, de l'eau, de l'acétone et de l'éthanol ; la phase liquide du flash étant essentiellement constituée d'eau. Le procédé selon la présente invention convient également pour la séparation de l'éthanol issu de la fermentation. La présente invention couvre également des dispositifs de mise en œuvre du procédé selon l'invention. Un dispositif préféré correspond à celui de la Figure 1 et comprend notamment un fermenteur (2) pourvu d'une arrivée des nutriments, gaz, moûts et autres (1 ) et d'un moyen d'évacuation du mout (3). Le mout est acheminé vers un moyen de séparation de la biomasse (4), tel qu'un module d'ultrafiltration. La biomasse est renvoyée au fermenteur (2) par un moyen d'acheminement approprié (8). Le liquide de fermentation débarrassé de sa biomasse est envoyée au système de l'évaporation flash (5), tel qu'un séparateur gaz-liquide (5). La phase liquide est acheminée vers le fermenteur (2) par un moyen approprié (7) et la phase gaz est alors évacuée vers un condenseur (6) qui sépare les incondensables résiduels des produits organiques d'intérêts. Ceux-ci seront alors isolés par une ou plusieurs techniques de séparations classiques. En sortie de condenseur (6) une partie du liquide peut être reflué vers la tête du séparateur gaz-liquide (5). The process according to the present invention is particularly suitable for the separation of biobutanol resulting from the fermentation of sugar cane molasses. In this case, the gaseous phase of step c) generally comprises CO 2 , H 2 , azeotrope / butanol / water, water, acetone and ethanol; the liquid phase of the flash essentially consisting of water. The process according to the present invention is also suitable for the separation of the ethanol resulting from the fermentation. The present invention also covers devices for implementing the method according to the invention. A preferred device corresponds to that of Figure 1 and comprises in particular a fermenter (2) provided with an arrival of nutrients, gas, musts and the like (1) and a means of evacuation of the mout (3). The mout is routed to a biomass separation means (4), such as an ultrafiltration module. The biomass is returned to the fermenter (2) by a suitable conveying means (8). The fermentation liquor freed of its biomass is sent to the flash evaporation system (5), such as a gas-liquid separator (5). The liquid phase is conveyed to the fermenter (2) by a suitable means (7) and the gas phase is then discharged to a condenser (6) which separates the remaining non-condensable organic products of interest. These will then be isolated by one or more conventional separation techniques. At the outlet of the condenser (6) a part of the liquid can be refluxed towards the head of the gas-liquid separator (5).
Un langage spécifique est utilisé dans la description de manière à faciliter la compréhension du principe de l'invention. Il doit néanmoins être compris qu'aucune limitation de la portée de l'invention n'est envisagée par l'utilisation de ce langage spécifique. Des modifications, améliorations et perfectionnements peuvent notamment être envisagés par une personne au fait du domaine technique concerné sur la base de ses propres connaissances générales. A specific language is used in the description so as to facilitate understanding of the principle of the invention. It should nevertheless be understood that no limitation of the scope of the invention is envisaged by the use of this specific language. In particular, modifications, improvements and improvements may be considered by a person familiar with the technical field concerned on the basis of his own general knowledge.
Le terme et/ou inclut les significations et, ou, ainsi que toutes les autres combinaisons possibles des éléments connectés à ce terme. The term and / or includes the meanings and, or, as well as all other possible combinations of elements connected to this term.
D'autres détails ou avantages de l'invention apparaîtront plus clairement au vu des exemples donnés ci-dessous uniquement à titre indicatif. PARTIE EXPERIMENTALE Other details or advantages of the invention will emerge more clearly in the light of the examples given below solely for information purposes. EXPERIMENTAL PART
Le dispositif testé correspond à celui de la Figure 1 et comprend notamment un fermenteur (2) d'une capacité de 1000 m3 et fonctionnant à une température de 38°C. Le fermenteur comprend du green juice concentré de cannes a sucre en début de fermentation. Le moyen de séparation (4) utilisé est un module d'ultrafiltration tangentielle. Le système de l'évaporation flash est un séparateur gaz-liquide (5) de type pot de flash. La phase liquide est acheminée vers le fermenteur (2) par un moyen approprié (7) et la phase gaz est alors évacuée vers un condenseur (6). Une partie de l'eau condensée de la phase gazeuse, débarassée des produits organiques est acheminée vers le fermenteur pour recyclage. Le cycle de production est de 200 heures. Le débit en sortie de l'ultrafiltration est réglée de manière à ce que par exemple 90 % de la masse soit recyclée vers le fermenteur par le moyen (8) et 10 % de la masse traverse les membranes du module d'ultrafiltration (4). La séparation flash est effectuée à une température de 30°C et une pression dans la phase gazeuse de 0,045 bar. The device tested corresponds to that of Figure 1 and comprises in particular a fermenter (2) with a capacity of 1000 m 3 and operating at a temperature of 38 ° C. The fermenter includes green juice concentrated with sugar cane at the beginning of fermentation. The separation means (4) used is a tangential ultrafiltration module. The system of flash evaporation is a gas-liquid separator (5) of flash pot type. The liquid phase is fed to the fermenter (2) by a suitable means (7) and the gas phase is then discharged to a condenser (6). Part of the condensed water of the gas phase, discarded organic products is sent to the fermenter for recycling. The production cycle is 200 hours. The flow rate at the outlet of the ultrafiltration is adjusted so that for example 90% of the mass is recycled to the fermenter by means (8) and 10% of the mass passes through the membranes of the ultrafiltration module (4). . The flash separation is carried out at a temperature of 30 ° C and a pressure in the gas phase of 0.045 bar.
Avec un taux de vaporisation de 40 % molaire ou 50 % massique dans le pot de flash, on obtient les flux entrant et sortant de l'évaporation flash suivants : With a vaporization rate of 40 mol% or 50% by mass in the flash pot, the following inflow and outflow flows are obtained:
Figure imgf000010_0001
Figure imgf000010_0001
% massique  % mass
On obtient une production de 1000 kg/h de butanol dans le fermenteur et de 1000 kg/h dans le flux sortant du condenseur (6). A production of 1000 kg / h of butanol in the fermenter and 1000 kg / h in the flow leaving the condenser (6) is obtained.
On observe ainsi une bonne séparation des produits organiques d'intérêt dans la phase gazeuse, avec un bon rendement, tout en assurant un équilibre thermique avec le recyclage du pieds de flash dans le fermenteur permettant d'éviter l'inhibition de la réaction dans le fermenteur. There is thus a good separation of the organic products of interest in the gas phase, with a good yield, while ensuring a thermal equilibrium with the recycling of the flash feet in the fermentor to avoid inhibition of the reaction in the fermenter.

Claims

REVENDICATIONS
1 . Procédé de séparation en continu des produits organiques d'une fermentation dans un fermenteur comprenant au moins les étapes suivantes : 1. Process for the continuous separation of organic products from a fermentation in a fermenter comprising at least the following steps:
a) prélèvement en cours de fermentation, d'une partie du moût du fermenteur ; b) séparation de la biomasse qui est renvoyée au fermenteur ; a) sampling during fermentation of part of the fermentor must; (b) separation of the biomass returned to the fermenter;
c) évaporation flash du liquide séparé à l'étape b), et obtention en phase gazeuse des produits organiques ; et c) flash evaporation of the liquid separated in step b), and obtaining in the gaseous phase of the organic products; and
d) isolation des produits organiques. d) insulation of organic products.
2. Procédé selon la revendication 1 , caractérisé en ce que la séparation de la biomasse est effectuée à l'étape b) avant d'effectuer l'évaporation flash de l'étape c). 2. Method according to claim 1, characterized in that the separation of the biomass is carried out in step b) before performing the flash evaporation of step c).
3. Procédé selon la revendication 1 ou 2, caractérisé en ce que la séparation de la biomasse à l'étape b) est effectué par filtration, ultrafiltration, décantation, centrifugation et/ou ultracentrifugation. 3. Method according to claim 1 or 2, characterized in that the separation of the biomass in step b) is carried out by filtration, ultrafiltration, decantation, centrifugation and / or ultracentrifugation.
4. Procédé selon l'une quelconque des revendications 1 à 3, caractérisé en ce que l'on procède à la séparation de la biomasse dans un séparateur gaz liquide utilisé pour effectuer l'évaporation flash. 4. Method according to any one of claims 1 to 3, characterized in that one proceeds to the separation of the biomass in a liquid gas separator used to perform the flash evaporation.
5. Procédé selon l'une quelconque des revendications 1 à 4, caractérisé en ce que l'évaporation flash est effectuée à une pression comprise entre 10 et 200 mbar. 5. Method according to any one of claims 1 to 4, characterized in that the flash evaporation is carried out at a pressure of between 10 and 200 mbar.
6. Procédé selon l'une quelconque des revendications 1 à 5, caractérisé en ce que la température lors de l'évaporation flash est comprise entre 10 et 40°C. 6. Method according to any one of claims 1 to 5, characterized in that the temperature during the flash evaporation is between 10 and 40 ° C.
7. Procédé selon l'une quelconque des revendications 1 à 6, caractérisé en ce que lors de l'évaporation flash le taux de vaporisation est compris entre 1 et 70 % massique. 7. Method according to any one of claims 1 to 6, characterized in that during flash evaporation the vaporization rate is between 1 and 70% by mass.
8. Procédé selon l'une quelconque des revendications 1 à 7, caractérisé en ce que la séparation lors l'évaporation flash est effectuée sans ajout de solvant particulier extérieur aux composés issus de la fermentation. 8. Process according to any one of claims 1 to 7, characterized in that the separation during flash evaporation is carried out without the addition of any particular external solvent to the compounds resulting from the fermentation.
9. Procédé selon l'une quelconque des revendications 1 à 8, caractérisé en ce que la phase aqueuse issue de la séparation flash est à une température inférieure à la température du fermenteur et est recyclée au fermenteur. 9. Process according to any one of claims 1 to 8, characterized in that the aqueous phase resulting from the flash separation is at a temperature below the temperature of the fermenter and is recycled to the fermenter.
10. Procédé selon l'une quelconque des revendications 1 à 9, caractérisé en ce que l'eau de la phase gazeuse issue de la séparation flash est condensée et est recyclée au fermenteur. 10. Process according to any one of claims 1 to 9, characterized in that the water of the gas phase resulting from the flash separation is condensed and is recycled to the fermenter.
1 1 . Procédé selon l'une quelconque des revendications 1 à 10, caractérisé en ce qu'il convient pour la séparation du biobutanol issu de la fermentation des mélasses de cannes a sucre. 1 1. Process according to any one of Claims 1 to 10, characterized in that it is suitable for the separation of the biobutanol obtained from the fermentation of molasses of sugar canes.
12. Dispositif pour la mise en œuvre du procédé selon l'une quelconque des revendications 1 à 1 1 . 12. Device for implementing the method according to any one of claims 1 to 1 1.
13. Dispositif selon la revendication 12 comprenant un fermenteur 2 pourvu d'une arrivée des nutriments, gaz, moûts et autres 1 et d'un moyen d'évacuation du mout 3, le mout est acheminé vers un moyen de séparation de la biomasse 4, tel qu'un module d'ultrafiltration, la biomasse est renvoyée au fermenteur 2 par un moyen d'acheminement approprié 8, le liquide de fermentation débarrassé de sa biomasse est envoyée au système de l'évaporation flash 5, tel qu'un séparateur gaz-liquide 5, la phase liquide est acheminée vers le fermenteur 2 par un moyen approprié 7 et la phase gaz est alors évacuée vers un condenseur 6 qui permettra la séparation des incondensables résiduels et des produits organiques d'intérêts. 13. Device according to claim 12 comprising a fermentor 2 provided with an arrival of nutrients, gas, musts and others 1 and a means of evacuation of the mout 3, the mout is routed to a means of separating the biomass 4 , such as an ultrafiltration module, the biomass is returned to the fermenter 2 by a suitable conveying means 8, the fermentation liquid freed of its biomass is sent to the flash evaporation system 5, such as a separator gas-liquid 5, the liquid phase is fed to the fermenter 2 by a suitable means 7 and the gas phase is then discharged to a condenser 6 which will separate residual incondensables and organic products of interest.
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